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综合实验研究优化白酒蒸馏工艺
综合实验研究优化白酒蒸馏工艺
综合实验研究优化白酒蒸馏工艺
a b s t r a c t
Systematic experiments were carried out to optimize the distillation process of Chinese liquor through an
industrial-scale distiller. Effect of the operation conditions on the yield and quality of the liquor, and varia-
tion of liquor components during distillation were investigated. The steam flowrate of 1.60 kg/min gives the best
yield and quality, suggesting there exists an optimal flowrate for the distillation. The yield and quality of the
liquor drops down obviously with the increase of bulk density, implying that the fermented grains should be
loosely packed. Increasing the bed height from 600 to 1250 mm enhances the yield and quality, indicating that
current distiller (commonly used bed height from 700 to 900 mm) has great potential of improvement. Adding
small amount of edible alcohol in the steam boiler is proven to increase the liquor yield, but excess amount
causes the quality degraded sharply. The liquor-vapor leaking is found to commonly occur at the initial stage
of distillation process and dramatically decrease the yield and quality. A simple method is proposed to elimi-
nate the leaking effectively. The gas chromatography analysis results show that the variation of flavor compounds
during distillation is closely related to their dissolving properties in ethanol.
© 2011 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
Keywords: Chinese liquor; Distillation; Optimization; Steam flowrate; Bulk density; Bed height
1. Introduction initial fermentation with the final blending. The goal of dis-
tillation is to extract the flavor compounds in the fermented
Chinese liquor is a popular alcoholic beverage with a con- grains. Therefore, the distillation process determines the yield
sumption of more than 4 million kilograms and sale revenue of and quality of the final product. For a long time, the research
about 500 billion Chinese Yuan (CNY) each year (China Brewing on Chinese liquor has been mainly focused on the species of
Industry Association and China Alcoholic Drinks Industry microorganism and the formations of flavor compounds dur-
Editorial Board, 2008). According to the aroma characteristics, ing the fermentation process (Shi et al., 2009; Xiang et al.,
Chinese liquor can be generally divided into five styles: the 2005; Zhang et al., 2005) and focused on the qualitative and
strong aroma style, light aroma style, sauce aroma style, rice quantitative analysis of the components in the final prod-
aroma style and miscellaneous aroma style (Fan and Qian, ucts (Fan and Qian, 2006a, 2006b; Zhu et al., 2007). However,
2006a). The manufacturing of Chinese liquor consists of three the distillation process has been less investigated and cur-
consecutive processes: fermentation, distillation and blend- rently applied distillation operation still follows the way that
ing. The fermentation is typically operated at 28–32 ◦ C for a it has been done in ancient time. Therefore, the investiga-
few months under anaerobic conditions in a solid state. After- tion of distillation process and improvement of its efficiency is
wards, the fermented grains are distilled with steam to extract an important subject in the present development of Chinese
ethanol and other flavor compounds. Finally, after being aged liquor.
for a period of time, these distillates are blended to yield the To optimize the distillation process, the following fac-
final product. The distillation plays a critical role to link the tors are important to be considered: (1) The steam flowrate,
∗
Corresponding author. Tel.: +86 28 85405209; fax: +86 28 85403397.
E-mail address: hwx@scu.edu.cn (W. Huang).
Received 27 March 2011; Received in revised form 29 August 2011; Accepted 19 December 2011
0960-3085/$ – see front matter © 2011 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
doi:10.1016/j.fbp.2011.12.005
food and bioproducts processing 9 0 ( 2 0 1 2 ) 392–398 393
the layer by layer mode, and the bulk density was in the 3. Results and discussion
range of 389.7–405.5 kg/m3 (higher bed with larger density).
The effect of the cross-steaming technique were discussed 3.1. Effect of the steam flowrate on the yield and
at five volume levels of edible alcohol, i.e., 0, 2, 4, 6 and 8 L, quality of the liquor
with keeping the bed height, steam flowrate and bulk density
fixed at 1250 mm, 1.60 kg/min and 389.7 kg/m3 , respectively. Fig. 2 shows the effect of the steam flowrate qm on the liquor
The added edible alcohol is composed of ethanol and water, yield m and quality. The yield in the study is calculated
in which the ethanol concentration is 95% by volume. based on 100 kg fermented grains, in which the concentra-
The distillates were continuously collected through the tion of ethanol is 60% by volume. As can be seen from
whole distillation process. The distillate samples were divided Fig. 2(a), increasing the steam flowrate from 1.20 to 1.60 kg/min
into two parts based on their ethanol concentrations in line enhances the yield of the liquor, but with further increasing
with the actual production: the distillates with ethanol con- the flowrate, the yield turns to decrease, especially after the
centration higher than 45% by volume were the effective steam flowrate exceeds to 2.30 kg/min. This phenomenon may
products, while those with ethanol concentration lower than come down to the thermodynamics and mass transfer dur-
45% by volume were the non-effective products for poor qual- ing the distillation process. The lower steam flowrate cannot
ity. The yield and quality of effective products are employed provide the thermal condition for full evaporation of ethanol
as the criterions for the distillation assessment and the effec- in the fermented grains, while the higher flowrate causes
tive products are called ‘liquor’ for short in this study. All the the grains to be pasted so that the mass diffusion within
distillation experiments were twice repeated and the results the grains become slower. Both situations results in lower
were expressed as mean data. liquor yield. Differently, with the increase in steam flowrate,
In order to better present the variation of flavor compounds a single decreasing trend for the yield was reported by some
during the distillation process, the dimensionless concentra- researchers (Pu, 2005a; Wan et al., 1998). This may be due to
tions C1 defined as C1 = ci,t /c̄i,t is introduced, where ci,j is the that their experimental conditions are limited to high steam
concentration of one specific flavor compound i in the dis- flowrates, not covering low steam flowrates. It can be observed
tillates obtained at j distillation time period and c̄i,t is the from Fig. 2(b) that the liquor distilled with the steam flowrate
arithmetic average value of ci,j . To express the effect of addition of 1.60 kg/min possesses the best quality. Therefore, from the
amount of edible alcohol into the boiler on the concentrations viewpoints of higher yield and better quality, there exists an
of flavor compounds in the liquor, the dimensionless concen- optimal steam flowrate for efficient distillation.
trations C2 is adopted. The definition of C2 (C2 = ci,V /c̄i,V ) is The liquor quality is mainly dependent on the concentra-
similar to that of C1 , where ci,V is the concentration of fla- tions of flavor compounds. Table 1 gives the concentrations
vor compound i in the liquors obtained at different addition of representative flavor compounds in the strong aroma type
amounts of edible alcohol in the steam boiler (V = 0, 2, 4, 6 liquor distilled from different steam flowrates. The ethanol
and 8 L) and c̄i,V is the arithmetic average value of ci,V . The concentration shows an upgrade tendency with the increase
dimensionless concentrations of the important flavor com- of steam flowrate from 1.20 to 1.60 kg/m3 , while it turns to
pounds in the strong aroma style liquor were calculated, such decrease for further increasing the flowrate. Furthermore, the
as, 1-propanol, 1-butanol, isobutanol, 1-hexanol, ethyl acetate, change of the concentration of flavor compounds presents
ethyl butanoic, ethyl hexanoate, ethyl lactate, acetic acid and close relationship with the dissolving properties in ethanol.
hexanoic acid. The concentrations of alcohol-soluble compounds, such as 1-
propanol, 1-butanol, ethyl acetate, ethyl butanoic and ethyl
hexanoate, exhibit similar trends with that of ethanol, while
2.3. Chemical and sensory analysis the concentration of water-soluble compounds, such as ethyl
lactate, acetic acid and hexanoic acid, are opposite to that of
Ethanol concentration was determined by a density meter ethanol.
(DMA 5000, Anton Paar, Graz, Austria), based upon the rela- Fig. 3 shows the dimensionless concentrations of flavor
tionship between the density of water–ethanol mixtures and compounds (C1 ) in the distillates obtained from different
the concentration of ethanol in the water–ethanol mixtures. distillation stages. The dimensionless concentrations (C1 )
An Agilent 6980 N (America) gas chromatography fitted with reflect the changes of the concentrations of flavor compounds
a flame ionization detector (FID) and a HP-INNOWax column
of 60 m × 0.25 mm × 0.25 m (Hewlett-Packard, Palo Alto, CA)
were used to quantify the flavor compounds. The experiment
was carried out at constant pressure, using nitrogen with the
flowrate of 1.8 ml/min as the carrier gas. Each concentrated
sample was injected at a split ratio of 1:50. The column tem-
perature was firstly programmed at 40 ◦ C for 4 min, followed by
increases of 2.5 ◦ C/min to 60 ◦ C and then 25 ◦ C/min to 120 ◦ C,
and increased from 10 ◦ C/min to 240 ◦ C, and held at 240 ◦ C for
4 min. Injector and detector temperatures were 240 ◦ C. The
analyses were performed in three replications.
The sensory quality was evaluated in duplicate by two well-
trained experts. They had more than 10 years experience in the
sensory analysis for Chinese liquor. Sensory attributes, includ-
ing taste, smell and aftertaste, were evaluated using a 10 point
hedonic scale, where 1 means dislike extremely and 10 means Fig. 2 – Effect of the steam flowrate (qm ) on the liquor yield
like extremely. (m) and quality.
food and bioproducts processing 9 0 ( 2 0 1 2 ) 392–398 395
Table 1 – Effect of the steam flowrate on the concentrations of the flavor compounds (g/L).
Compounds Steam flowrate, qm (kg/min)
Fig. 5 – Effect of the bed height (H) on the liquor yield (m) Fig. 6 – Effect of the cross-steaming on the liquor yield (m)
and quality. and quality.
Table 3 – Effect of the bed height on the concentrations of the flavor compounds (g/L).
Compounds H (mm)
during the distillation process are found to be closely related Pu, L.L., 2005a. Study on Distillation Technology of Luzhou Daqu
to their dissolving properties in ethanol. Liquor. Tianjin University of Science and Technology, Tianjin.
The industrial-scaled experiments in the study offer an Pu, L.L., 2005b. Study on the effects of the height of fermented
grains layer on liquor distillation and liquor quality.
important direction for the practical production, especially for
Liquor-Making Science & Technology 128, 42–45.
the enhancement and improvement of distillation process and Shi, E., Huang, W.X., Xiao, Z.Y., Tang, X.Y., Xu, R.Q., Zeng, F.J., 2007.
equipment. Study on improvement of the quality in Chinese new-type
liquor by pervaporation with polydimethylsiloxane
membrane. Journal of Food Process Engineering 30, 38–50.
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